白果仁及炒白果仁内源性有害成分分析

Analysis of endogenous harmful components in ginkgo seed kernel and fried ginkgo seed kernel

以白果仁、炒白果仁为试验材料,采用HPLC法测定总银杏酸,色谱柱为YMC-Triart C18(4.6mm×150mm,5μm),流动相为0.1%三氟乙酸的乙腈溶液-0.1%三氟乙酸的水溶液,检测波长为310nm,流速为1.0mL/min;采用HPLC法测定4′-O-甲基吡哆醇(MPN)和4′-O-甲氧基吡哆醇-5′-葡萄糖苷(MPNG),色谱柱为YMC-Triart C18(4.6mm×150mm,5μm),流动相为甲醇-去离子水,检测波长为328nm,流速为1.0mL/min。采用顶空气相色谱(HS-GC)法对氢氰酸进行限度检查。结果表明,总银杏酸的平均回收率为101.17%、RSD为4.57%(n=6)、定量限为12.18ng、检测限为4.87ng;MPN平均回收率为103.14%、RSD为4.80%(n=6)、定量限为5.94ng、检测限为2.38ng;MPNG平均回收率为103.54%、RSD为3.05%(n=6)、定量限为11.20ng、检测限为4.48ng;氢氰酸定量限为10ng、检测限为3.5ng。建立的方法专属性强、重复性好,灵敏度高,可用于白果仁、炒白果仁中内源性有害成分的检测。

Ginkgo seed kernel and fried ginkgo seed kernel were used as experimental materials for the determination of total ginkgolic acid using HPLC.The chromatographic column was YMC-Triart C18(4.6mm×150mm,5μm).The mobile phase was acetonitrile solution with 0.1%trifluoroacetic acid-0.1%trifluoroacetic acid aqueous solution,with a detection wavelength of 310nm and a flow rate of 1.0mL/min;4′-O-methyl pyridoxine(MPN)and 4′-O-methoxy pyridoxin-5′-glucoside(MPNG)were determined by HPLC on YMC Triart C18(4.6mm×150mm,5μm).The mobile phase was methanol deionized water,with a detection wavelength of 328nm and a flow rate of 1.0mL/min.Headspace gas chromatography(HS-GC)was used to perform a limit check on hydrocyanic acid.The results showed that the average recovery rate of total ginkgolic acid was 101.17%,RSD was 4.57%(n=6),the quantification limit was 12.18ng,and the detection limit was 4.87ng;the average recovery rate of MPN was 103.14%,RSD was 4.80%(n=6),the quantification limit was 5.94ng,and the detection limit was 2.38ng;the average recovery rate of MPNG was 103.54%,RSD was 3.05%(n=6),the quantification limit was 11.20ng,and the detection limit was 4.48ng;the quantitative limit of hydrocyanic acid was 10ng,and the detection limit was 3.5ng.The established method had strong specificity,good repeatability,and high sensitivity,and could be used for the detection of endogenous harmful components in ginkgo seed kernel and fried ginkgo seed kernel.